The recent introduction of acetylene-terminated polyimides to produce cured reaction products which are stable at very high temperatures of 450.degree. C. and up has created an interest and need to produce the polyimides at attractive and competitive costs. The prime difficulty in the preparation of the acetylene-terminated polyimides which are described, for example, in U.S. Pat. No. 3,845,018 and U.S. Pat. No. 3,879,349, both to Norman Bilow et al., is the preparation of the monomers which include in one instance the preparation of meta-aminophenylacetylene (APA). The process of this invention relates to improved procedures for the preparation of precursors to nitrophenylacetylene, which itself is a precursor to APA.